The objective of this work is to present the optimization of SMB operating conditions under the fixed performance of high purity (over 99%), which takes mass transfer effect into account. The parameters for the numerical calculation were used by our previous work [1,2] of binary separation of aqueous mixture of glucose and fructose. The equilibrium isotherm was linear and the mass transfer was described by LDF approximation. The single parameter of Stanton number was used for the mass transfer effect. The result of our work was compared with that of the triangle theory [3]. For the sake of this procedure, an analytical solution for a TMB mode was suggested and compared with the simulated result of SMB mode. The advantage of the TMB model with the mass transfer effect was the rapid determination of the flow conditions of each zone for the required purity of extract and raffinate.